CN109836148B - Permanent magnetic ferrite material without La and Co elements and preparation method thereof - Google Patents
Permanent magnetic ferrite material without La and Co elements and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of ferrite materials. The invention discloses a permanent magnetic ferrite material without La and Co elements, which mainly comprises Fe2O3、SrCO3、SiO2、Y2O3、Cr2O3MgO and the like; the invention also discloses a preparation method of the permanent magnetic ferrite material without La and Co elements, which comprises the steps of material preparation, ball milling, presintering, crushing, compounding, molding, calcining, post-treatment and the like. According to the invention, the formula is adjusted, the process is optimized, ferrite particles can be pre-sintered at 1000-1150 ℃, the size of the pre-sintered powder grains is uniform and is closer to a spherical shape, and the magnetic performance of the sintered magnet obtained after secondary ball milling, molding and sintering is higher. According to the invention, the sintered ferrite permanent magnet material with high coercivity and high remanence is prepared by optimizing the material components, improving the uniformity of ferrite grains and effectively improving the intrinsic coercivity of the material under the condition that La and Co elements are not added.
Description
Technical Field
The invention relates to the technical field of ferrite materials, in particular to a permanent magnetic ferrite material without La and Co elements and a preparation method thereof.
Background
The M-type permanent magnetic ferrite is an oxide with ferrimagnetism, has good magnetic property and outstanding cost performance, and is widely applied to the fields of household appliance motors, sensors, office equipment, automobile motors, medical equipment and the like.
Since the nineties of the last century, strontium ferrite gradually develops Sr-La-Co series and Sr-Ca-La-Co series strontium ferrite on the basis of La-Co ion substitution, and stable hexagonal ferrite crystals, a larger magnetocrystalline anisotropy constant K1 and a higher material saturation magnetization Ms value are obtained. However, in recent two years, rapid development of the lithium ion battery industry has driven rapid increase of the price of Co resources, and as a strategic resource, the supply of Co itself is limited, and it is expected that the price of Co will still remain at a high level with the development of new energy automobile industry in China in the future. Therefore, the development of the high-performance permanent magnetic ferrite without Co element has important significance, can partially replace the existing strontium ferrite material containing LaCo element, reduces the cost of raw materials, and improves the product competitiveness.
Disclosure of Invention
In order to solve the problems, the invention provides a sintered ferrite permanent magnet material with high coercivity and high remanence, which is prepared by optimizing the components of the material, improving the uniformity of ferrite grains, effectively improving the intrinsic coercivity of the material and not adding La and Co elements.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a permanent magnetic ferrite material without La and Co elements is mainly prepared from the following raw materials in percentage by weight: fe2O385-88 wt% of SrCO311 to 14 wt% of SiO20.2 to 0.6 wt.% of Y2O30.04-0.2 wt% of Cr2O30.05-0.2 wt% and 0-0.6 wt% MgO.
Preferably, the average particle size of each raw material is 5 μm or less.
Preferably, SiO2The particle size of (A) is 100 to 500 nm.
A preparation method of a permanent magnetic ferrite material without La and Co elements comprises the following steps:
a) preparing materials: preparing the raw materials according to the components and the content;
b) ball milling: mixing the raw materials, and then carrying out ball milling and crushing;
c) pre-burning: pre-burning the ball-milled raw materials to prepare a pre-sintered material;
d) crushing: crushing the pre-sintered material;
e) and (3) compounding: adding an additive into the pulverized pre-sintering material, and performing ball milling and wet mixing to obtain slurry;
f) molding: dehydrating the slurry and forming in a magnetic field to obtain a formed body;
g) and (3) calcining: calcining the formed body at 1100-1300 ℃ for 0.5-2.0 hours to prepare a permanent magnetic ferrite material without La and Co elements;
h) and (5) post-treatment.
Preferably, in the ball milling in the step b), the weight ratio of the raw materials, the milling balls and the water is 1: (12-16): (1-2), the ball milling speed is 50-90 rpm, and the ball milling time is 3-7 hours.
Preferably, in the step c), the pre-sintering temperature is 1000-1200 ℃, and the pre-sintering time is 2-4 hours.
Preferably, in the step d) of crushing, the pre-sintered material is crushed into particles of 4-6 microns.
Preferably, the additive is made of CaCO in the step e) of compounding3、SiO2And dispersant composition, CaCO3The addition amount of the additive is 0.5-0.7 wt% of the pre-sintering material, and SiO2The addition amount is 0.15-0.25 wt% of the pre-sintering material, and the addition amount of the dispersing agent is 0.15-0.25 wt% of the pre-sintering material; CaCO3And SiO2The particle size of (A) is 100 to 500 nm.
Preferably, the ball milling time is 14 to 18 hours during the compounding in the step e).
Preferably, during the step f) of forming, the slurry is dehydrated to the water content of 30-40 wt%, and is formed in a magnetic field of 8000-12000 Oe, and the forming pressure is 4.5-5.5 MPa.
Preferably, in the step g), during calcination, the formed body is firstly kept at the temperature of 110-130 ℃ for 0.8-1.2 hours, then the temperature is raised to 1100-1300 ℃ at the temperature raising rate of 110-130 ℃ per hour, the temperature is kept for 0.5-2.0 hours, and then the formed body is cooled.
Preferably, the post-treatment in the step h) comprises grinding and cleaning the prepared permanent magnetic ferrite material without La and Co elements, and then preserving the heat for 20-28 hours at 20-25 ℃.
The existing permanent magnetic ferrite technology mainly comprises the steps of adding oxides of La and Co for ion substitution and searching for slurry particle miniaturization to obtain the high-performance permanent magnetic ferrite, but because La and Co are expensive resources and fine particles are not beneficial to magnet molding, the development of the low-cost high-performance permanent magnetic ferrite technology is necessary. The key technology of the invention is as follows: 1) the formula of the rare-earth-free permanent magnetic ferrite is optimized, the pre-sintering process is improved, the addition of magnesium oxide is beneficial to obtaining that the pre-sintered material is a single ferrite phase at a lower temperature of 1000-1150 ℃, the grains of the pre-sintered material are fine and uniform, the average grain size is about 0.5 mu m, and the integrity of the original grains is kept as far as possible in the subsequent secondary ball milling process, so that the magnet has higher comprehensive magnetic performance; 2) after the nano silicon dioxide and the nano calcium carbonate are added in the sintering process, the grain nucleation points are increased, and the uniform grain size is beneficial to obtaining the high-performance permanent magnetic ferrite.
Therefore, the invention has the following beneficial effects:
according to the invention, the formula is adjusted, the process is optimized, ferrite particles can be pre-sintered at 1000-1150 ℃, the size of the pre-sintered powder grains is uniform and is closer to a spherical shape, and the magnetic performance of the sintered magnet obtained after secondary ball milling, molding and sintering is higher.
According to the invention, the sintered ferrite permanent magnet material with high coercivity and high remanence is prepared by optimizing the material components, improving the uniformity of ferrite grains and effectively improving the intrinsic coercivity of the material under the condition that La and Co elements are not added.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present invention, all the equipments and materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
A preparation method of a permanent magnetic ferrite material without La and Co elements comprises the following steps:
a) preparing materials: proportioning according to weight percentage, wherein Fe2O3Content 85wt％，SrCO3Content 13.4 wt%, SiO2Content 0.6 wt%, Y2O30.2 wt% of Cr2O30.2 wt% of MgO and 0.6 wt% of SiO, the average particle diameter of each raw material being 5 μm or less2Has a particle diameter of 100 nm;
b) ball milling: mixing the raw materials, and then carrying out ball milling and crushing; during ball milling, the weight ratio of the raw materials, the grinding balls and water is 1: 12: 1, the ball milling speed is 50rpm, and the ball milling time is 3 hours;
c) pre-burning: pre-burning the ball-milled raw materials to prepare a pre-sintered material; when in presintering, the presintering temperature is 1000 ℃, and the presintering time is 2 hours;
d) crushing: crushing the pre-sintered material into 4-micron particles;
e) and (3) compounding: adding an additive into the pulverized pre-sintered material, and carrying out ball milling for 14 hours to obtain slurry through wet mixing; the additive being made of CaCO3、SiO2And dispersant composition, CaCO3The addition amount of the additive is 0.5 wt% of the pre-sintering material, and the SiO content2The addition amount is 0.15 wt% of the pre-sintering material, and the addition amount of the dispersant is 0.15 wt% of the pre-sintering material; CaCO3And SiO2Has a particle diameter of 100 nm;
f) molding: dehydrating the slurry to a water content of 30 wt%, and forming in a magnetic field of 8000Oe at a forming pressure of 4.5MPa to obtain a formed body;
g) and (3) calcining: firstly, keeping the temperature of a formed body at 110 ℃ for 0.8 hour, then heating to 1100 ℃ at the heating rate of 110 ℃ per hour, keeping the temperature for 0.5 hour, and then cooling;
h) and (3) post-treatment: and grinding and cleaning the prepared permanent magnetic ferrite material without La and Co elements, and then preserving heat for 20 hours at 20 ℃.
Example 2
A preparation method of a permanent magnetic ferrite material without La and Co elements comprises the following steps:
a) preparing materials: proportioning according to weight percentage, wherein Fe2O388 wt.% of SrCO311% by weight of SiO2Content 0.31 wt%, Y2O30.04 wt% of Cr2O30.05 wt% of MgO and 0.6 wt% of SiO, the average particle diameter of each raw material being 5 μm or less2Has a particle size of 500 nm;
b) ball milling: mixing the raw materials, and then carrying out ball milling and crushing; during ball milling, the weight ratio of the raw materials, the grinding balls and water is 1: 16: 2, the ball milling speed is 90rpm, and the ball milling time is 7 hours;
c) pre-burning: pre-burning the ball-milled raw materials to prepare a pre-sintered material; when in presintering, the presintering temperature is 1200 ℃, and the presintering time is 4 hours;
d) crushing: pulverizing the pre-sintering material into particles of 6 microns;
e) and (3) compounding: adding an additive into the pulverized pre-sintered material, and performing ball milling for 18 hours to obtain slurry through wet mixing; the additive being made of CaCO3、SiO2And dispersant composition, CaCO3The addition amount of the additive is 0.7 wt% of the pre-sintering material, and the SiO content2The addition amount is 0.25 wt% of the pre-sintering material, and the addition amount of the dispersant is 0.25 wt% of the pre-sintering material; CaCO3And SiO2Has a particle size of 500 nm;
f) molding: dehydrating the slurry until the water content is 40 wt%, and forming in a 12000Oe magnetic field to obtain a formed body, wherein the forming pressure is 5.5 MPa;
g) and (3) calcining: firstly, keeping the temperature of the formed body at 130 ℃ for 1.2 hours, then heating to 1300 ℃ at the heating rate of 130 ℃ per hour, keeping the temperature for 2.0 hours, and then cooling;
h) and (3) post-treatment: and grinding and cleaning the prepared permanent magnetic ferrite material without La and Co elements, and then preserving heat for 28 hours at 25 ℃.
Example 3
A preparation method of a permanent magnetic ferrite material without La and Co elements comprises the following steps:
a) preparing materials: proportioning according to weight percentage, wherein Fe2O3Content 86.4 wt%, SrCO3Content 13 wt%, SiO2Content 0.1 wt%, Y2O30.1 wt% of Cr2O30.1 wt% of MgO and less than 5 micron of CaCO3And SiO2Particle diameter ofIs 300 nm;
b) ball milling: mixing the raw materials, and then carrying out ball milling and crushing; during ball milling, the weight ratio of the raw materials, the grinding balls and water is 1: 14: 1.5, the ball milling speed is 70rpm, and the ball milling time is 5 hours;
c) pre-burning: pre-burning the ball-milled raw materials to prepare a pre-sintered material; when in pre-sintering, the pre-sintering temperature is 1100 ℃, and the pre-sintering time is 3 hours;
d) crushing: crushing the pre-sintered material into particles of 5 microns;
e) and (3) compounding: adding an additive into the pulverized pre-sintered material, and carrying out ball milling for 16 hours to obtain slurry through wet mixing; the additive being made of CaCO3、SiO2And dispersant composition, CaCO3The addition amount of the additive is 0.6wt percent of the pre-sintering material and SiO2The addition amount is 0.2 wt% of the pre-sintering material, and the addition amount of the dispersant is 0.2 wt% of the pre-sintering material; CaCO3And SiO2Has a particle size of 300 nm;
f) molding: dehydrating the slurry until the water content is 35 wt%, and forming in a 10000Oe magnetic field to obtain a formed body, wherein the forming pressure is 5 MPa;
g) and (3) calcining: firstly, keeping the temperature of the formed body at 120 ℃ for 1.0 hour, then heating to 1200 ℃ at the heating rate of 120 ℃ per hour, keeping the temperature for 1.5 hours, and then cooling;
h) and (3) post-treatment: and grinding and cleaning the prepared permanent magnetic ferrite material without La and Co elements, and then preserving heat for 24 hours at 22 ℃.
Example 4
A preparation method of a permanent magnetic ferrite material without La and Co elements comprises the following steps:
a) preparing materials: proportioning according to weight percentage, wherein Fe2O387.6 wt% SrCO3Content 12.11 wt%, SiO2Content 0.2 wt%, Y2O30.04 wt% of Cr2O30.05 wt% of MgO, 5 μm or less of the average particle diameter of each raw material, SiO2Has a particle diameter of 200 nm;
b) ball milling: mixing the raw materials, and then carrying out ball milling and crushing; during ball milling, the weight ratio of the raw materials, the grinding balls and water is 1: 14: 1.5, the ball milling speed is 70rpm, and the ball milling time is 5 hours;
c) pre-burning: pre-burning the ball-milled raw materials to prepare a pre-sintered material; when in pre-sintering, the pre-sintering temperature is 1100 ℃, and the pre-sintering time is 3 hours;
d) crushing: crushing the pre-sintered material into particles of 5 microns;
e) and (3) compounding: adding an additive into the pulverized pre-sintered material, and carrying out ball milling for 16 hours to obtain slurry through wet mixing; the additive being made of CaCO3、SiO2And dispersant composition, CaCO3The addition amount of the additive is 0.6wt percent of the pre-sintering material and SiO2The addition amount is 0.2 wt% of the pre-sintering material, and the addition amount of the dispersant is 0.2 wt% of the pre-sintering material; CaCO3And SiO2Has a particle diameter of 200 nm;
f) molding: dehydrating the slurry until the water content is 35 wt%, and forming in a 10000Oe magnetic field to obtain a formed body, wherein the forming pressure is 5 MPa;
g) and (3) calcining: firstly, keeping the temperature of the formed body at 120 ℃ for 1 hour, then heating the formed body to 1200 ℃ at the heating rate of 120 ℃ per hour, keeping the temperature for 1 hour, and then cooling the formed body;
h) and (3) post-treatment: and grinding and cleaning the prepared permanent magnetic ferrite material without La and Co elements, and then preserving heat for 24 hours at 23 ℃.
Example 5
A preparation method of a permanent magnetic ferrite material without La and Co elements comprises the following steps:
a) preparing materials: proportioning according to weight percentage, wherein Fe2O387.5 wt% SrCO3Content 12.3 wt%, SiO2Content 0.11 wt%, Y2O30.04 wt% of Cr2O30.05 wt% of MgO, 5 μm or less of the average particle diameter of each raw material, SiO2Has a particle diameter of 200 nm;
b) ball milling: mixing the raw materials, and then carrying out ball milling and crushing; during ball milling, the weight ratio of the raw materials, the grinding balls and water is 1: 14: 1.5, the ball milling speed is 70rpm, and the ball milling time is 5 hours;
c) pre-burning: pre-burning the ball-milled raw materials to prepare a pre-sintered material; when in pre-sintering, the pre-sintering temperature is 1050 ℃, and the pre-sintering time is 3 hours;
d) crushing: crushing the pre-sintered material into particles of 5 microns;
e) and (3) compounding: adding an additive into the pulverized pre-sintered material, and carrying out ball milling for 16 hours to obtain slurry through wet mixing; the additive being made of CaCO3、SiO2And dispersant composition, CaCO3The addition amount of the additive is 0.6wt percent of the pre-sintering material and SiO2The addition amount is 0.2 wt% of the pre-sintering material, and the addition amount of the dispersant is 0.2 wt% of the pre-sintering material; CaCO3And SiO2Has a particle diameter of 200 nm;
f) molding: dehydrating the slurry until the water content is 35 wt%, and forming in a 10000Oe magnetic field to obtain a formed body, wherein the forming pressure is 5 MPa;
g) and (3) calcining: firstly, keeping the temperature of the formed body at 120 ℃ for 1 hour, then heating the formed body to 1180 ℃ at the heating rate of 120 ℃ per hour, keeping the temperature for 1 hour, and then cooling the formed body;
h) and (3) post-treatment: and grinding and cleaning the prepared permanent magnetic ferrite material without La and Co elements, and then preserving heat for 24 hours at 23 ℃.
Examples 6 to 10
Examples 6-10 the data in Table 1 below are different from example 5 except that the other parameters are the same as those shown in example 5.
Table 1:
comparative example 1
Comparative example 1 except for CaCO used as additive3、SiO2The grain diameter of the material is micron-sized, namely CaCO with the grain diameter of 10 microns is adopted3、SiO2Except for the differences, the other parameters were the same as those shown in example 5.
And (3) performance testing:
magnetic property tests were conducted on the magnets obtained in examples 1 to 10 and comparative example 1.
The magnetic property test results are shown in table 2 below.
TABLE 2
From the comparison between the example 4 and the comparative example 1, it can be known that the secondary addition of the nano silica and the nano calcium carbonate is helpful to improve the Br and Hcj of the permanent magnetic ferrite material, mainly because the nano particles are increased, the nucleation points are increased, the growth of the crystal grains is hindered, and the ferrite crystal grains are uniform and fine in size in the secondary nucleation process.
From the comparison of examples 5 to 10, it can be known that when magnesium oxide of not more than 0.8 wt% is added, the pre-sintering temperature is reduced to 1150 ℃, and the sintered permanent magnetic ferrite with higher magnetic performance and without La and Co elements can be obtained.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (9)
1. A permanent magnetic ferrite material without La and Co elements is characterized by being mainly prepared from the following raw materials in percentage by weight: fe2O385-88 wt% of SrCO311 to 14 wt% of SiO20.1 to 0.6 wt.% of Y2O30.04-0.2 wt% of Cr2O30.05 to 0.2 wt% of MgO, 0 to 0.6 wt% of MgO;
the preparation process of the permanent magnetic ferrite material without La and Co elements is as follows:
a) preparing materials: preparing the raw materials according to the components and the content;
b) ball milling: mixing the raw materials, and then carrying out ball milling and crushing;
c) pre-burning: pre-burning the ball-milled raw materials to prepare a pre-sintered material;
d) crushing: crushing the pre-sintered material;
e) and (3) compounding: adding an additive into the pulverized pre-sintering material, and performing ball milling and wet mixing to obtain slurry;
f) molding: dehydrating the slurry and forming in a magnetic field to obtain a formed body;
g) and (3) calcining: calcining the formed body at 1100-1300 ℃ for 0.5-2.0 hours to prepare a permanent magnetic ferrite material without La and Co elements;
h) post-treatment;
when said step e) is compounding, the additive is made of CaCO3、SiO2And dispersant composition, CaCO3The addition amount of the additive is 0.5-0.7 wt% of the pre-sintering material, and SiO2The addition amount is 0.15-0.25 wt% of the pre-sintering material, and the addition amount of the dispersing agent is 0.15-0.25 wt% of the pre-sintering material; the CaCO3And SiO2The particle size of (A) is 100 to 500 nm.
2. The La and Co element-free permanent magnetic ferrite material according to claim 1, wherein:
the average particle size of each raw material is less than 5 micrometers.
3. The La-Co-free permanent magnetic ferrite material according to claim 1 or 2, wherein:
the SiO2The particle size of (A) is 100 to 500 nm.
4. The preparation method of the permanent magnetic ferrite material without La and Co elements according to claim 1 is characterized by comprising the following steps:
a) preparing materials: preparing the raw materials according to the components and the content;
b) ball milling: mixing the raw materials, and then carrying out ball milling and crushing;
c) pre-burning: pre-burning the ball-milled raw materials to prepare a pre-sintered material;
d) crushing: crushing the pre-sintered material;
e) and (3) compounding: adding an additive into the pulverized pre-sintering material, and performing ball milling and wet mixing to obtain slurry;
f) molding: dehydrating the slurry and forming in a magnetic field to obtain a formed body;
g) and (3) calcining: calcining the formed body at 1100-1300 ℃ for 0.5-2.0 hours to prepare a permanent magnetic ferrite material without La and Co elements;
h) and (5) post-treatment.
5. The method for preparing the permanent magnetic ferrite material without La and Co elements according to claim 4, wherein the method comprises the following steps: during ball milling in the step b), the weight ratio of the raw materials, the grinding balls and the water is 1: (12-16): (1-2), the ball milling speed is 50-90 rpm, and the ball milling time is 3-7 hours.
6. The method for preparing the permanent magnetic ferrite material without La and Co elements according to claim 4, wherein the method comprises the following steps: and c) when pre-burning is carried out in the step c), the pre-burning temperature is 1000-1200 ℃, and the pre-burning time is 2-4 hours.
7. The method for preparing the permanent magnetic ferrite material without La and Co elements according to claim 4, wherein the method comprises the following steps: and f) dehydrating the slurry to a water content of 30-40 wt% during forming, and forming in a magnetic field of 8000-12000 Oe at a forming pressure of 4.5-5.5 MPa.
8. The method for preparing the permanent magnetic ferrite material without La and Co elements according to claim 4, wherein the method comprises the following steps: and g) during calcination, firstly keeping the temperature of the formed body at 110-130 ℃ for 0.8-1.2 hours, then heating to 1100-1300 ℃ at the temperature rise rate of 110-130 ℃ per hour, keeping the temperature for 0.5-2.0 hours, and then cooling.
9. The method for preparing the permanent magnetic ferrite material without La and Co elements according to claim 4, wherein the method comprises the following steps: and the post-treatment in the step h) comprises grinding and cleaning the prepared permanent magnetic ferrite material without La and Co elements, and then preserving heat for 20-28 hours at 20-25 ℃.
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| CN107010937A (en) * | 2017-04-26 | 2017-08-04 | 宿州学院 | One kind contains Cu2+W-type ferrite material and its preparation |
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